Реакция #595370
ord-41752e8eda6a478d996396309c9f08f6
Уравнение реакции
4-bromo-2-fluoro-5-methylbenzoic acid
SOCl2
CH3OH
→
title compound
methyl 4-bromo-2-fluoro-5-methylbenzoate
Реагенты
Нет
Условия реакции
Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ДругоеThe solvent was removed in vacuo
- 2workup.ADDITIONthe residue was diluted with EtOAc
- 3Промывкаwashed with H2O, brine
- 4Сушкаdried over anhydrous Na2SO4
- 5Концентрированиеconcentrated
- 6ПромывкаThe resulting crude solid was washed with PE
Методика
To a solution of 4-bromo-2-fluoro-5-methylbenzoic acid (i-2a) (1.87 g, 8 mmol) in CH3OH (50 mL) at 0° C. was added SOCl2 (6 mL, 80 mmol) dropwise. Then the mixture was heated to 80° C. for 2 h. The solvent was removed in vacuo and the residue was diluted with EtOAc and washed with H2O, brine, dried over anhydrous Na2SO4, and concentrated. The resulting crude solid was washed with PE to give the title compound as a yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.80 (1H, d), 7.37 (1H, d), 3.92 (3H, s), 2.39 (3H, s).